CN101666762B - Detecting method of liquid-phase generation characteristics of sintered iron ore - Google Patents
Detecting method of liquid-phase generation characteristics of sintered iron ore Download PDFInfo
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Abstract
The invention provides a detecting method of a liquid-phase generation characteristic of sintered iron ore. The invention proposes that a cone-shaped method is adopted to detect the liquid-phase generation characteristic according to the principle that the material deformation and liquid-phase generation have close relation. The liquid-phase generation characteristic comprises the temperature, speed and quantity of liquid-phase formation, the characteristic temperature of liquid-phase formation is detailed as liquid-phase starting generating temperature Ts, liquid-phase complete generation temperature Te and liquid-phase free flow temperature Tf, and the characteristic temperature is obtained by automatic recognition of an image processing software according to cone-shaped changing characteristic shot by the camera. The liquid-phase generation average speed is calculated by a formula v=1000/(Te-Ts); and the liquid-phase generation amount is represented by shrinkage ratio of cone-shaped area at the temperature of 1280 DEG C and cone-shaped area at the temperature of 1000 DEG C. The detecting method is characterized by fast detecting speed, simple measurement method and accurate detecting result and can establish corresponding relation with the quality index of sintered ore.
Description
Technical field
The present invention relates to a kind of detection method of liquid-phase generation characteristics of sintered iron ore,, be used for estimating the iron ore quality and the performance that are applied to sintering by detecting the liquid-phase generation characteristics index of iron ore in becoming the ore deposit process.
Background technology
Existing valuation of iron ore method, major part all are to weigh the quality of iron ore according to the chemical constitution of iron ore and physical property.But angle from sintering fine fodder technology, it is far from being enough only estimating iron ore from normal temperature characteristics such as chemical constitution, size composition, pellet performances, the one-tenth ore deposit performance of iron ore also is important measurement index under the high temperature, because the structure and the mineral composition that become the ore deposit process influence sintering deposit, with the quality of sintering deposit extremely close getting in touch arranged, thus the output of sintering deposit, quality and sintering energy consumption depend on iron ore under the condition of high temperature to a greater extent become the ore deposit performance.
But at present people are not enough to the one-tenth ore deposit behavior understanding of iron ore in sintering process, thereby can't be fully and correctly hold inner link between iron ore kind and the sintering effect.Causing existing ore-proportioning method all is to select iron ore according to the chemical constitution and the physical property of iron ore basically, joins the ore deposit by sintering cup test then.Because the understanding that sinters the ore deposit process into is lacked the degree of depth, be unfavorable for the high efficiency management of SINTERING PRODUCTION and the correct prediction of sinter quality, thereby join the ore deposit and have blindness, cause having wasted great amount of manpower and material resources.
If the high-temperature physics chemical characteristic that iron ore is reflected in sintering process can reflect by becoming the ore deposit performance index, and set up relation between itself and sintering deposit yield and quality, the energy consumption, just can on purpose various iron ores reasonably be selected and use, realize Optimization Ore Matching truly.Simultaneously these indexs can be the key property of understanding and grasping iron ore, judge its sintering character, select technological parameter and for iron and steel enterprise's buying iron ore, be optimized and join the ore deposit and instruct SINTERING PRODUCTION that strong rationale is provided.
Go back the system neither one standard of comparison, science at present and estimate the one-tenth ore deposit performance of sintering iron-bearing material, even do not propose to sinter into ore deposit performance detection content clearly.From sintering mechanism, sinter the ore deposit process into and comprise that solid phase reaction, liquid phase in the sintering process generate and the not molten ore of bonding and three main processes of condensation-crystallization.By experimental study, the result shows that liquid phase is the fixed basis of sintering deposit moulding, is into important contents in the performance of ore deposit.Liquid phase is the bonding phase of sintering deposit, and not molten solid particle is bonded to piece, guarantees that sintering deposit has certain intensity, so the quantity of liquid phase and character are the important factor in order of sinter strength.The quantity and the sintering process gas penetration potential of liquid phase are closely related simultaneously, thereby affect the sintering deposit productive rate.And liquid phase generation temperature, formation speed and sintering energy consumption have strong correlation, if can form the required liquid phase of sintering at low temperatures fast, then can reduce sintering temperature, thereby reduce sintering energy consumption.
Above-mentioned sintering liquid phase is generalized into two class features, is respectively liquid-phase generation characteristics and liquid phase bonding characteristic.Liquid-phase generation characteristics comprises that liquid phase generates temperature, formation speed, generation quantity, and what the present invention relates to is the detection method of liquid-phase generation characteristics.
The present situation of liquid-phase generation characteristics detection method and the problem of existence:
The many complexities that in sintering process, generate liquid phase with assimilation performance characterization iron ore of detection technique in the past.The assimilation performance be meant iron ore in sintering process with the reaction capacity of CaO.Generally speaking, iron ore assimilation performance is high more, then easy more generation liquid phase in sintering process.For research following representational method is arranged with voltinism:
1. the detection method of University of Science ﹠ Technology, Beijing's Wu Shengli etc., be that Iron Ore Powder and the pure CaO reagent of analysis are made fine-powdered (～100 order), under certain pressure, be pressed into the little cake of breeze of diameter 8mm and the little cake of CaO of diameter 25mm respectively, then the little cake sample of Iron Ore Powder is placed on the little cake sample of CaO, put in the miniature sintering experiment device of people and carry out roasting by certain sintering schedule.To generate the reactant that is slightly larger than little cake one circle of Iron Ore Powder on little cake of breeze and the little cake surface of contact of CaO is the assimilation feature, measures the temperature and time that reaches this assimilation feature, estimates the assimilative capacity of different Iron Ore Powder and CaO with this.This method can detect the temperature that iron ore and CaO begin to react, but the response situation that can not observe iron ore under continuous temperature can only be observed its assimilation feature at the temperature spot that is interrupted, and causes the workload tested big; Owing to detecting the temperature that begins to react, not strong simultaneously to the generating feature directiveness of sintering process liquid phase.
2. another common method is that raw material is pressed into agglomerate, sintering under certain temperature and atmosphere, by detecting the assimilation performance that ore deposit phase composition in the agglomerate reflects iron ore, the different researcher's operating conditionss or the equipment of use can be different, but basic principle is similar.Japan FumioMATSLJNO and Takeo HARA-DA be with various raw material pulverizing to 0.125mm, mix the little cake that the back is pressed into compound Φ 15mm * 10mm, be put into then be heated in the electric furnace temperature required, by microscope, X-diffraction, EPMA observe the mineral phase structure in the little cake at last.The J.A.Whiteman of the Li-Heng in Taiwan and Sheffield university be with various raw material pulverizing to 0.125mm, be pressed into the agglomerate of Φ 6mm * 6mm after the mixing, be put into then and be heated to temperature requiredly in the electric furnace, feed N in the roasting process
2, Air, CO, CO
2Mixed gas is simulated sintering atmosphere.The research method of the C.E.Loo of BHP company, various raw material pulverizing are mixed the back and are pressed group to 0.125mm, are put into then to be heated to temperature requiredly in the infrared heating furnace, feed N in the roasting process
2, Air, CO, CO
2Mixed gas is simulated sintering atmosphere, detects the formation situation of calcium ferrite in the agglomerate then.These class methods need be worn into the sintering agglomerate mating plate and observe microstructure, and the mineral composition of statistics agglomerate; Perhaps agglomerate is ground, therefore the ore deposit phase with in the X-diffraction detection agglomerate can not realize fast detecting.And agglomerate cools off behind sintering, and liquid phase is constantly separated out crystal in cooling procedure, becomes branch constantly to change, and the ore deposit of therefore detecting agglomerate is the generation situation of liquid phase in the reaction-sintered process really mutually.
State same voltinism that detection method surveys and all fail comprehensively to embody the generation behavior of sintering process liquid phase, and have the testing process complicated problems, very unobvious with the corresponding relation of sintering effect yet.Therefore, develop a kind of method of all sidedly, scientifically weighing the sintering process liquid-phase generation characteristics, and realize accurate detection, seem particularly important.
Summary of the invention
Technical matters to be solved by this invention has provided a kind of detection method of liquid-phase generation characteristics of sintered iron ore, and this method adopts the taper sintering process to detect the iron ore liquid-phase generation characteristics.
For achieving the above object, technical scheme of the present invention is:
A kind of detection method of liquid-phase generation characteristics of sintered iron ore is characterized in that, may further comprise the steps:
1) batching: select iron ore and calcium oxide for use, the mass ratio that calcium oxide accounts for iron ore and calcium oxide total amount is 10%～20%, makes iron ore drying and granularity less than 0.074mm; With smashing to pieces after the calcium oxide digestion, add in the iron ore mixing to; Add entry again and mix, the moisture quality accounts for 7-10%; Get compound;
2) sintering and detection: compound is pressed into pyrometric cone, and with pyrometric cone roasting under air atmosphere, programming rate is (10 ± 2) ℃/min; Obtain iron ore liquid-phase generation characteristics parameter according to the profile variation situation of pyrometric cone in the intensification roasting process, concrete grammar is as follows:
Liquid phase begins to generate that temperature T s begins to become circle for the pyrometric cone tip or the temperature of correspondence when crooked;
When liquid phase generates temperature T e fully and refers to that the pyrometric cone cone is bent to awl point and touches supporting plate or cone shrink the temperature of capping correspondence when spherical;
Liquid phase flows freely temperature T f and is meant that pyrometric cone is melted into one or is launched into the temperature of height when the following thin layer of 1.5mm;
It is v=1000/ (Te-Ts) that liquid phase generates average velocity;
Liquid phase growing amount η is that the shrinkage rates with the lateralarea of 1280 ℃ of following pyrometric cones characterizes; Be specially η=(S
1000-S
1280)/S
1000* 100%; S wherein
1280The area of a side of the pyrometric cone of camera picked-up when being 1280 ℃, S
1000One area of the pyrometric cone of camera picked-up when being 1000 ℃.
Temperature when height/end at the beginning of the pyrometric cone, height was for (123 ± 3) % is that liquid phase begins to generate temperature T s; When the wide/high temperature during for (145 ± 5) % of hat spheroid is that liquid phase generates temperature T e fully; Temperature when pyrometric cone is melted into wide/height for (1100 ± 20) % is that liquid phase flows freely temperature T f.
The morphological feature of monitoring pyrometric cone by the CCD camera in real time changes.
The size characteristic of described pyrometric cone is to be the equilateral triangle of the length of side 7mm end, and the pyrometric cone height is 20mm, and wherein a rib is perpendicular to the bottom surface.
The beneficial effect that the present invention has is:
The present invention generates according to material distortion and liquid phase and exists this principle of substantial connection to propose employing coning detection iron ore liquid-phase generation characteristics.Liquid-phase generation characteristics comprises temperature, speed and the quantity that liquid phase forms, the characteristic temperature that liquid phase forms is embodied in that liquid phase begins to generate temperature (Ts), liquid phase generates temperature (Te) fully and liquid phase flows freely temperature (Tf), and characteristic temperature is discerned acquisition according to the taper variation characteristic that camera takes automatically by image processing software.Liquid phase generates average velocity and calculates with formula v=1000/ (Te-Ts); The liquid phase growing amount is to characterize with the shrinkage rates that 1280 ℃ of inferior pyramidal areas are compared 1000 ℃ of inferior pyramidal areas.
This method has been considered generation temperature, speed and three characteristics of growing amount of liquid phase simultaneously, compares with the detection of voltinism more comprehensively, and can reflect the situation of change that iron ore liquid phase in whole sintering process generates.
This method is at same equipment, with once just detecting three characteristics that liquid phase generates in the test, have therefore that measuring method is simple, detection speed soon, the testing result characteristic of accurate.
The liquid-phase generation characteristics that this method detects can be set up corresponding relation with sintering deposit yield and quality index, therefore has science and practicality.
Therefore, this method is a kind of method of all sidedly, scientifically weighing the sintering process liquid-phase generation characteristics, and realizes accurate detection.
Description of drawings
Model and synoptic diagram and the installation supporting plate of Fig. 1 for making pyrometric cone; Wherein a figure is a mould of making pyrometric cone; B figure is the pyrometric cone synoptic diagram, CB=BD=CD=7mm wherein, AD ⊥ Δ BCD, AD=20mm; C figure is the supporting plate that pyrometric cone is installed, and 5 pyrometric cones can be installed simultaneously, and installation method is over against camera with side Δ ABC.
Fig. 2 is the heating furnace synoptic diagram; Wherein: the 1-thermopair; The 2-carborunbum tube; The 3-pyrometric cone; 4-corundum boat; The 5-furnace shell; 6-corundum outer tube; 7-corundum inner sleeve; 8-foamed alumina insulating brick; 9-electroplax sheet; The 10-viewport.
Fig. 3 surveys the liquid-phase generation characteristics process flow diagram for coning;
Fig. 4 surveys liquid phase generating feature temperature synoptic diagram for coning; [wherein 4 groups of images from left to right represent respectively that unreacted, liquid phase begin to generate, liquid phase generates fully and the triangular pyramidal morphological feature of liquid phase when flowing freely];
Fig. 5 shrinks synoptic diagram [wherein figure left and right sides image is respectively the triangular pyramidal side view of 1000 degree and 1280 when spending] for pyrometric cone.
Embodiment
Detect content
Detect the formation characteristic of sintered iron ore, mainly be obtain temperature height that iron ore generates liquid phase, form the speed of liquid phase and under sintering temperature the growing amount of liquid phase, generate the complexity of liquid phase by the detection reflection iron ore of these features.Therefore, the formation characteristic of liquid phase comprises that liquid phase begins to generate temperature, liquid phase and generates fully that temperature, liquid phase flow freely temperature, liquid phase generates average velocity, liquid phase growing amount.
Detection method
(1) coning is measured the principle of liquid-phase generation characteristics.When material in the process that heats up gradually, material is owing to melt and produce distortion, but the fusing degree of the degree reaction mass of distortion.For sharp-featured material, therefore the phenomenon of easier its distortion of observation makes triangular pyramidal with material.By measuring the deformation extent of pyrometric cone in temperature-rise period, detect the liquid-phase generation characteristics of iron ore.
(2) method of coning simulation sintering.
1) simulation sintered material.Iron ore sintering process generation complex physico-chemical, because the factor of contact conditions, solid phase reaction at first takes place with CaO in iron ore, and the low melting point that these solid phase reactions generate is the guide that liquid phase generates, and calcium ferrite is most important bonding phase system in the final sintering deposit.The reaction of iron ore and CaO can reflect the generation of sintering process liquid-phase system, and therefore batching is selected the generative process of iron ore and two kinds of material simulations of CaO sintering liquid phase.
2) simulation sintering process.Two aspects of process control that mainly comprise temperature and atmosphere.Programming rate is (10 ± 2) ℃/min, and calcination atmosphere is an oxidizing atmosphere, promptly heats under the atmosphere of air.
Checkout equipment
(1) taper making and erecting equipment (see figure 1)
(2) heater element (see figure 2)
(3) real-time checkout equipment of image and process software
Adopt the situation of change of CCD camera real time record whole experiment intermediate cam awl, and utilize advanced image recognition technology to judge the feature that pyrometric cone changes, recording feature temperature and pyrometric cone form realize identification automatically.And automatically store significance map picture in the experiment, so that further check and analyze.
Adopt TT﹠C software that the temperature-rise period of high temperature furnace is controlled.
Operating process
The experiment process of coning is seen Fig. 3.
Coning is surveyed the method for operating of liquid phase characteristics:
(1) raw material is prepared.In drying baker, more than the dry 2h, iron ore is fully dehydrated iron ore to be measured; Iron ore is finely ground to granularity less than 0.074mm.
(2) batching.Take by weighing the 50g iron ore, the unslaked lime addition calculates according to proportioning.To fully smash to pieces behind the quicklime slaking, add abundant mixing in the ore deposit to.With addition of a certain amount of water, make the suitable compacting of mixture moisture pyrometric cone then, general moisture is 7 ~ 10%.
(3) preparation of pyrometric cone and installation: in model, suppress pyrometric cone, and it is installed on the supporting plate.
Experimental phenomena and feature
(1) liquid phase forms the experimental phenomena of characteristic temperature and the judgement (synoptic diagram is seen Fig. 4) of feature thereof:
1) liquid phase begins to generate temperature (Ts): refer to that the pyrometric cone tip begins to become circle or crooked temperature, judgment criterion is that just height/end, height was (123 ± 3) % to pyrometric cone;
2) liquid phase generates temperature (Te) fully: refer to when the pyrometric cone cone is bent to awl point and touches supporting plate or cone is shunk the temperature of capping when spherical, judgment criterion be hat spherical wide/highly be (145 ± 5) %;
3) liquid phase flows freely temperature (Tf): be to be melted into one or to be launched into the temperature of height during at the following thin layer of 1.5mm when pyrometric cone, judgment criterion be thin layer wide/highly be (1100 ± 20) %.
(2) liquid phase growing amount and liquid phase generate the sign of average velocity
1) sign of liquid phase growing amount
Form liquid phase in material, shrinkage phenomenon can take place in material under the effect of power such as capillary force, gravity, see Fig. 5.It is many more that liquid phase produces, and the ratio of contraction is big more.Therefore the shrinkage rates that (is generally 1280 ℃) with pyrometric cone under sintering temperature characterizes the quantity that liquid phase generates.The pyrometric cone of deviating to cause of water of crystallization shrinks in the ore deposit in order to get rid of, and is benchmark with the area of 1000 ℃ of following pyrometric cones.The computing formula of shrinkage rates is as follows:
η＝(S
1000-S
1280)/S
1000×100％；
S
1280--the area of the tapered side Δ ABC (seeing b figure among Fig. 1) of camera picked-up under 1280 ℃ the temperature;
S
1000--S
1000The area of the tapered side Δ ABC of camera picked-up when being 1000 ℃.
2) liquid phase generates the sign of average velocity
Liquid phase generates consuming time longly more from beginning to be generated to fully, illustrates that formation speed is slow more, and the definition liquid phase generates average velocity and is:
v＝1000/(Te-Ts)％/min。
Embodiment:
Below two groups of experiments, one group is the Australia ore deposit, one group is the India ore deposit.Every group of test has two kinds of ore deposits, and from identical country, and their chemical constitution is close with size composition.The research liquid-phase generation characteristics is to the influence of sintering deposit yield and quality index.
(1) be example with two kinds of Australia's powder, as can be seen from Table 1, Australia's powder-1 and Australia's powder-2 are close substantially in chemical constitution and size composition.Two kinds of Australia's ore deposit liquid-phase generation characteristics see Table 2 to the influence of sintering deposit output, quality, energy consumption index, as can be known, the liquid phase of Australia's powder-2 begins to generate that temperature, liquid phase generate temperature fully, liquid phase flows freely temperature is all lower than Australia powder-1, and formation speed is faster than Australia powder, and best dosage of coke Australia powder-1 height; Australia's powder-2 liquid phase formation amount under 1280 ℃ temperature is more than Australia's powder-1, and sintered ore rotary drum strength, yield rate are than Australia powder-1 height.
(2) be example with two kinds of India's powder, as can be seen from Table 1, India's powder-1 and India's powder-2 are close substantially in chemical constitution and size composition.Two kinds of India's ore deposit liquid-phase generation characteristics see Table 2 to the influence of sintering deposit output, quality, energy consumption index, as can be known, the liquid phase of India's powder-2 begins to generate that temperature, liquid phase generate temperature fully, liquid phase flows freely temperature is all lower than India powder-1, and formation speed is faster than India powder, and best dosage of coke India powder-1 height; India's powder-2 liquid phase formation amount under 1280 ℃ temperature is more than India's powder-1, and sintered ore rotary drum strength, yield rate are than India powder-1 height.
The physical and chemical performance of table 1 iron ore
The liquid-phase generation characteristics in table 2 import ore deposit and sintering deposit yield and quality
Claims (4)
1. the detection method of a liquid-phase generation characteristics of sintered iron ore is characterized in that, may further comprise the steps:
1) batching: select iron ore and calcium oxide for use, the mass ratio that calcium oxide accounts for iron ore and calcium oxide total amount is 10%～20%, makes iron ore drying and granularity less than 0.074mm; With smashing to pieces after the calcium oxide digestion, add in the iron ore mixing to; Add entry again and mix, the moisture quality accounts for 7-10%; Get compound;
2) sintering and detection: compound is pressed into pyrometric cone, and with pyrometric cone roasting under air atmosphere, programming rate is (10 ± 2) ℃/min; Obtain iron ore liquid-phase generation characteristics parameter according to the profile variation situation of pyrometric cone in the intensification roasting process, concrete grammar is as follows:
Liquid phase begins to generate that temperature T s begins to become circle for the pyrometric cone tip or the temperature of correspondence when crooked;
When liquid phase generates temperature T e fully and refers to that the pyrometric cone cone is bent to awl point and touches supporting plate or cone shrink the temperature of capping correspondence when spherical;
Liquid phase flows freely temperature T f and is meant that pyrometric cone is melted into one or is launched into the temperature of height when the following thin layer of 1.5mm;
It is v=1000/ (Te-Ts) that liquid phase generates average velocity;
Liquid phase growing amount η is that the shrinkage rates with the lateralarea of 1280 ℃ of following pyrometric cones characterizes; Be specially η=(S
1000-S
1280)/S
1000* 100%; S wherein
1280The area of the tapered side of the pyrometric cone of camera picked-up when being 1280 ℃, S
1000The area of the same tapered side of the pyrometric cone of camera picked-up when being 1000 ℃.
2. the detection method of liquid-phase generation characteristics of sintered iron ore according to claim 1 is characterized in that, the temperature when height/end at the beginning of the pyrometric cone, height was for (123 ± 3) % is that liquid phase begins to generate temperature T s; When the wide/high temperature during for (145 ± 5) % of hat spheroid is that liquid phase generates temperature T e fully; Temperature when pyrometric cone is melted into wide/height for (1100 ± 20) % is that liquid phase flows freely temperature T f.
3. the detection method of liquid-phase generation characteristics of sintered iron ore according to claim 1 is characterized in that, the morphological feature of monitoring pyrometric cone by the CCD camera in real time changes.
4. the detection method of liquid-phase generation characteristics of sintered iron ore according to claim 1 is characterized in that, the size characteristic of described pyrometric cone is to be the equilateral triangle of the length of side 7mm end, and the pyrometric cone height is 20mm, and wherein a rib is perpendicular to the bottom surface.
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| CN105372273A (en) * | 2015-11-24 | 2016-03-02 | 北京科技大学 | Method for measuring iron ore powder and CaO assimilation reaction performance |
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| CN113820343A (en) * | 2021-08-18 | 2021-12-21 | 首钢集团有限公司 | Method for detecting high-temperature liquid phase generation proportion of sinter |
| CN114486993A (en) * | 2021-12-28 | 2022-05-13 | 武钢集团昆明钢铁股份有限公司 | Method for detecting assimilation temperature of iron ore powder |
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